反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[C:4]([N+:12]([O-:14])=[O:13])[CH:3]=1.Cl.[C:16]([O-])([O-])=O.[Na+].[Na+]>CO>[CH3:16][O:10][C:9](=[O:11])[CH2:8][C:5]1[CH:6]=[CH:7][C:2]([Br:1])=[CH:3][C:4]=1[N+:12]([O-:14])=[O:13]参加物
5
反応条件
- 温度
- 85 °C
実験手順
A solution of (4-bromo-2-nitro-phenyl)-acetic acid (5.00 g, 19.2 mmol) in methanol (100 mL) is treated with conc. HCl (1.0 mL). The mixture is stirred at 85° C. for 16 hours and cooled to room temperature. The mixture is neutralized with aqueous Na2CO3 and concentrated under reduced pressure. The residue is extracted with ethyl acetate (50 mL×2), and the combined organic layers are dried over sodium sulfate and concentrated under reduced pressure to provide the title compound (5.27 g, 100%) as a brown solid.
後処理
- temperaturecooled to room temperature
- concentrationconcentrated under reduced pressure
- extractionThe residue is extracted with ethyl acetate (50 mL×2)
- dry with materialthe combined organic layers are dried over sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-39c68c4774554e8bb89b8a0df36ed1e9
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07863302B2
関連ノート
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